- 1, 3-propane sultone methyl fluoro derivative as well as preparation method and application thereof
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The invention relates to a preparation method of a 1, 3-propane sultone methyl fluoro derivative, which comprises the following steps: 1) taking 3-butene-2-alcohol and sodium hydrogen sulfite as raw materials, taking peroxide as an initiator, carrying out addition reaction in an ammonia water solution, after full reaction, reducing pressure, heating and concentrating until the material is thick, and acidizing by using concentrated hydrochloric acid, cooling to room temperature, filtering and concentrating filtrate to be viscous, transferring the concentrated filtrate into a vacuum reaction kettle, continuously flash-evaporating, dehydrating and cyclizing under a high-temperature vacuum condition, and rectifying a crude product to obtain 3-methyl-PS; and 2) preparing the methyl fluoro derivative: fully mixing 3-methyl-PS with dichloromethane, adding a fluorinating agent, fully reacting, and removing dichloromethane under reduced pressure to obtain the methyl fluoro derivative. The preparation method has the advantages that 3-methyl-PS is successfully prepared, the 3-methyl-PS can be directly fluorinated, the product structure is clear and single, no by-product is generated, and the methyl fluoro derivative has an obvious effect of enhancing the performance of a lithium battery when being used as an electrolyte additive of the lithium battery.
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Paragraph 0022-0030
(2021/09/26)
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- Synthesis method of 2, 4-butane sultone
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The invention discloses a synthesis method of 2, 4-butane sultone, which comprises the following steps: 1, dissolving 1, 3-propane sultone in a first organic solvent under the protection of inert gas in the whole process, then adding sodium hydrogen in batches, and heating to 40-50 DEG C after the sodium hydrogen is added; 2, dropwise adding a methylation reagent, and carrying out heat preservation reaction after dropwise adding; and 3, cooling to room temperature, adding ice water and a second organic solvent for extraction, and carrying out negative pressure rectification on the second organic solvent layer to obtain the final product 2, 4-butane sultone. The synthesis method has the advantages of low raw material cost, simple operation steps, mild reaction conditions, few reaction steps, easiness in purification and the like.
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Paragraph 0030-0032
(2021/06/21)
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- Synthesis of a series of sulfinic acid analogs of GABA and evaluation of their GABA(B) receptor affinities
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A series of γ-aminobutyric acid (GABA) 1 analogs was prepared in which the carboxylic acid group of GABA was replaced with a sulfinic acid group and their affinity for the GABA(B) receptor investigated.
- Carruthers, Nicholas I.,Spitler, James M.,Wong, Shing-Chun,Blythin, David J.,Chen, Xiao,Shue, Ho-Jane,She, Hoyan S.,Lee, Joe F.,Rizzo, Charles,Ting, Pauline C.,West Jr., Robert E.
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p. 3059 - 3064
(2007/10/03)
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- Lithium aluminum hydride-aluminum hydride reduction of sultones
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Lithium aluminum hydride-aluminum hydride reduction of secondary and tertiary (C-O) substituted γ-sultones or α-alkyl-β'-hydroxy γ-sultones yields mercapto alcohols and mercapto diols, respectively, in fair to good yield.These products result from S-O cleavage of the sultone ring.Primary sultones and α-dialkyl-β'-hydroxy γ-sultones give predominantly C-O cleavage to form sulfonic acid derivatives. β-Sultones are much less reactive toward the mixed hydride, and refluxing in dioxane is required for their reduction.
- Smith, Michael B.,Wolinsky, Joseph
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p. 101 - 106
(2007/10/02)
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